ragga (Newbee)
10-20-00 01:23
No 61608
      synth of cyclohexyamine  Bookmark   

Cyclohexane
or
Cyclohexanone
-----> Cycloheylamine

Cycloheylamine was used in the Shulgin synth of 3,4,5-Trimethoxyphenethylamine, and seems to be the only difficult chemical to aquire. is there another chemical substitute to use in this synth? or is there an intermediate to it with a synth without even harder precursurs?
 
 
 
 
    Rhodium
(Chief Bee)
10-20-00 12:04
No 61760
      Re: synth of cyclohexyamine  Bookmark   

3,4,5-trimethoxynitrostyrene:

A solution of 40 cc of nitromethane and 100 g. of trimethoxybenzaldehyde in 200 ml alcohol is cooled to 0C and while it is stirred
mechanically there is introduced a solution of 45 g. pure potassium hydroxide in 45 ml water and 90 cc methanol at the rate of about one
drop per second, care being taken that the temperature does not rise. Fifteen minutes after the addition is completed the solution is
poured into 500 cc concentrated hydrochloric acid mixed with sufficient fee to assure its presence throughout the slow addition and to
maintain the temperature of -10C. The precipitated nitrostyrene is separated by filtration and washing and may be purified by
recrystallizing from 700 ml alcohol. The pale yellow plates which melt at 120-121C are obtained in a yield of approximately 78% of theory.

Ref: J Prakt Chem 137, 339 (1933)



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    ragga
(Newbee)
10-20-00 16:13
No 61803
      Re: synth of cyclohexyamine  Bookmark   

thanks!
this is just what i needed!
can i use IPA for the alcohol excluding 90cc of methonal?
 
 
 
 
 
    Rhodium
(Chief Bee)
10-21-00 16:12
No 62066
      Re: synth of cyclohexyamine  Bookmark   

Yes, you can probably use IPA instead of methanol.


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